CN113877643B - 检测水污染的纤维素3d增强拉曼光谱微流芯片及其应用 - Google Patents

检测水污染的纤维素3d增强拉曼光谱微流芯片及其应用 Download PDF

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CN113877643B
CN113877643B CN202111098641.1A CN202111098641A CN113877643B CN 113877643 B CN113877643 B CN 113877643B CN 202111098641 A CN202111098641 A CN 202111098641A CN 113877643 B CN113877643 B CN 113877643B
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王丹
姚凯彬
黄映洲
唐军
郭昌川
雒鑫伟
郑颖
康一骏
韩水平
吴小祥
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Chongqing University
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Abstract

本发明公开了一种检测水污染的纤维素3D增强拉曼光谱微流芯片，第一步，材料及设备准备；第二步，纳米纤维素线净化；第三步，纤维素线羧化处理；第四步，纤维素线AgNPs银纳米粒子的合成：先将羧化处理后的纤维素线放入硝酸银溶液中浸泡，再放入硼氢化钠溶液中浸泡，得到表面泛黄的3D包裹银纳米的纤维素线，通入去离子水缓缓冲洗去除未反应的杂质，最后放入干燥箱中干燥；第五步，在微流管道中放入一根3D包裹银纳米的纤维素线作为微流控芯片，通过plasma等离子体键合，将微流控芯片键合在载玻片上。同时，本发明还公开了检测水污染的纤维素3D增强拉曼光谱微流芯片的应用。低成本、高灵敏度、制作工艺简便，能对水中污染物进行快速、精确检测。

Description

检测水污染的纤维素3D增强拉曼光谱微流芯片及其应用
技术领域
本发明涉及水中污染物成分检测技术领域，具体涉及到一种纤维素3D增强拉曼光谱微流芯片，及其应用。
背景技术
拉曼光谱提供了指纹光谱，可实现分子的无标记传感。然而，由于光谱分辨率低，拉曼散射信号的整体强度太弱难以实现复用传感，需要开发能够以超高灵敏度和高光谱分辨率检测分子的原位技术。表面增强拉曼光谱(SERS)是一种这样的技术，它具有高灵敏度。当SERS与微流体通道耦合时，可以实现连续SERS检测。为了获得SERS集成的微流控平台，SERS活性材料应在微流控通道内制造。目前已经开发了几种沉积方法来制造SERS活性金属纳米结构，例如电子束蒸发器、激光沉积、Langmuir-Blodgett技术和热蒸发。然而，这些方法对器材及材料要求较高，并且生成的SERS活性材料与待测样接触面积仅有一面，接触面积较小影响芯片的灵敏度。
近年来，发展中国家因工业快速发展而造成的重金属污染日益严重，已成为一个严重的环境问题。因此，检测水和食品中痕量污染物对于保护环境和人类健康至关重要。对于这些有毒物质的现场检测，最好选择封闭的环境。然而，只有少数研究专注于在封闭的微流体通道中制造金属纳米结构阵列，因为制造这种设备既复杂又耗时。纳米结构以允许在微通道中进行测量，胶体金属纳米粒子必须注入通道中，同时还需要小心控制流速和在此类系统中精心设计的微流体芯片。
发明内容
针对上述问题，本发明旨在提供一种低成本、高灵敏度、制作工艺简便的3D增强拉曼光谱微流芯片，能对水中污染物进行快速、精确检测。
为此，本发明所采用的技术方案为：一种检测水污染的纤维素3D增强拉曼光谱微流芯片，包括以下步骤：
第一步，材料及设备准备；
硝酸银、硼氢化钠、氢氧化钠、羧化壳聚糖、醋酸、去离子水；
纳米纤维素线、微流管道、真空干燥箱；
第二步，纳米纤维素线净化：将纳米纤维素线用1％-3％w/v的氢氧化钠溶液在80±5℃水浴加热搅拌3±0.5h，去除木质素和半纤维素；再用去离子水洗涤纳米纤维素线，然后保存在去离子水中；
第三步，纤维素线羧化处理：将羧化壳聚糖溶解于醋酸中配置成羧化酸溶液，配置比例为：1g羧化壳聚糖：50ml1％v/v醋酸；再将净化后的纳米纤维素线从去离子水中取出放入羧化酸溶液中，在60±5℃下搅拌50-70min，然后保存在去离子水中；
第四步，纤维素线AgNPs银纳米粒子的合成：先将羧化处理后的纤维素线放入浓度为1mol/L的硝酸银溶液中浸泡5-20min，再取出纤维素线放入浓度为1mol/L的硼氢化钠溶液中浸泡5-20min，得到表面泛黄的3D包裹银纳米的纤维素线，通入去离子水缓缓冲洗去除未反应的杂质，最后放入干燥箱中干燥；
第五步，在微流管道中放入一根3D包裹银纳米的纤维素线作为微流控芯片，通过plasma等离子体键合，将微流控芯片键合在载玻片上。
作为上述方案的优选，所述去离子水为0.8％-0.9％w/w。
进一步优选为，第二步中，采用浓度为2％w/v的氢氧化钠溶液，水浴温度为80℃，搅拌时间为3h。
进一步优选为，第三步中，采用的羧化壳聚糖1g，醋酸50ml，温度为60℃，搅拌60min。
进一步优选为，第四步中，1mol/L的硝酸银、1mol/L的硼氢化钠溶液各5ml，均提前15min制备以保持新鲜。
同时，本发明还公布了一种上述的检测水污染的纤维素3D增强拉曼光谱微流芯片的应用，将污水通入检测水污染的纤维素3D增强拉曼光谱微流芯片中，再对吸附后的微流控芯片进行SERS检测。
作为上述方案的优选，SERS检测采用的拉曼激光波长633nm，积分时间为20s，拉曼检测参数为0.7mw。
本发明的有益效果：
(1)采用纳米纤维素线依次浸泡硝酸银溶液和硼氢化钠溶液，进行银纳米粒子的3D包裹，相比传统的通过微流泵依次向微流管道中以20微升/分钟的规定速度缓慢通入上述两种溶液，不需要小心控制流速，操作更加轻松简便；
(2)采用浸泡的方式，能使银纳米粒子在纤维素线外形成3D包裹，纤维素线状立体结构可以360度吸附银颗粒，同时纤维素线具有褶皱性表面，增大了吸附银颗粒的面积，羧化处理的纤维素线也更容易与银颗粒相结合，再将其置入微流管道中作为微流控芯片，能增大芯片与待测样品的接触面积，提高灵敏度和检测精准度；而传统的直接向微流管道中通入硝酸银溶液和硼氢化钠溶液的方式，由于重力作用，仅能在微流管道底部合成银纳米粒子，造成芯片与待测样品的接触面积小，检测灵敏度和精准度不高；
(3)此方法针对于水中污染物的检测不会影响水质发生变化，检测方法简单，对器材及材料要求较低，因此具有普遍性。
附图说明
图1为纤维素线的SEM图。
图2为微流管道模拟图。
图3为用于含三聚氰胺污水检测时，传统微流控芯片与本发明SERS信号对比图。
具体实施方式
下面通过实施例并结合附图，对本发明作进一步说明：
结合图1—图3所示，一种检测水污染的纤维素3D增强拉曼光谱微流芯片，包括以下步骤：
第一步，材料及设备准备。
硝酸银、硼氢化钠、氢氧化钠、羧化壳聚糖、醋酸、去离子水。
纳米纤维素线、微流管道、真空干燥箱。
第二步，纳米纤维素线净化。
将纳米纤维素线用1％-3％w/v的氢氧化钠溶液在80±5℃水浴加热搅拌3±0.5h，去除木质素和半纤维素；再用去离子水洗涤纳米纤维素线，然后保存在去离子水中；
优选为：采用0.8％-0.9％w/w的去离子水，采用浓度为2％w/v的氢氧化钠溶液，水浴温度为80℃，搅拌时间为3h。
第三步，纤维素线羧化处理：将羧化壳聚糖溶解于醋酸中配置成羧化酸溶液，配置比例为：1g羧化壳聚糖：50ml1％v/v醋酸；再将净化后的纳米纤维素线从去离子水中取出放入羧化酸溶液中，在60±5℃下搅拌50-70min，然后保存在去离子水中。
优选为：采用的羧化壳聚糖1g，醋酸50ml，温度为60℃，搅拌60min。
第四步，纤维素线AgNPs银纳米粒子的合成。
先将羧化处理后的纤维素线放入浓度为1mol/L的硝酸银溶液(0.01689g/ml)中浸泡5-20min，再取出纤维素线放入浓度为1mol/L的硼氢化钠溶液(0.00398g/ml)中浸泡5-20min，得到表面泛黄的3D包裹银纳米的纤维素线，通入去离子水缓缓冲洗去除未反应的杂质，最后放入干燥箱中干燥。
优选为：1mol/L的硝酸银、1mol/L的硼氢化钠溶液各5ml，均提前15min制备以保持新鲜。
第五步，在微流管道中放入一根3D包裹银纳米的纤维素线作为微流控芯片，通过plasma等离子体键合，将微流控芯片键合在载玻片上。
上述检测水污染的纤维素3D增强拉曼光谱微流芯片的应用，将污水通入检测水污染的纤维素3D增强拉曼光谱微流芯片中，再对吸附后的微流控芯片进行SERS检测。
优选为：SERS检测采用的拉曼激光波长633nm，积分时间为20s，拉曼检测参数为0.7mw。

Claims (7)

1.一种检测水污染的纤维素3D增强拉曼光谱微流芯片，其特征在于，包括以下步骤：
第一步，材料及设备准备；
硝酸银、硼氢化钠、氢氧化钠、羧化壳聚糖、醋酸、去离子水；
纳米纤维素线、微流管道、真空干燥箱；
第二步，纳米纤维素线净化：将纳米纤维素线用1%-3%w/v的氢氧化钠溶液在80±5°C水浴加热搅拌3±0.5h，去除木质素和半纤维素；再用去离子水洗涤纳米纤维素线，然后保存在去离子水中；
第三步，纤维素线羧化处理：将羧化壳聚糖溶解于醋酸中配置成羧化酸溶液，配置比例为：1g羧化壳聚糖：50ml1%v/v醋酸；再将净化后的纳米纤维素线从去离子水中取出放入羧化酸溶液中，在60±5°C下搅拌50-70min，然后保存在去离子水中；
第四步，纤维素线AgNPs银纳米粒子的合成：先将羧化处理后的纤维素线放入浓度为1mol/L的硝酸银溶液中浸泡5-20min，再取出纤维素线放入浓度为1mol/L的硼氢化钠溶液中浸泡5-20min，得到表面泛黄的3D包裹银纳米的纤维素线，通入去离子水缓缓冲洗去除未反应的杂质，最后放入干燥箱中干燥；
第五步，在微流管道中放入一根3D包裹银纳米的纤维素线作为微流控芯片，通过plasma等离子体键合，将微流控芯片键合在载玻片上。
2.按照权利要求1所述的检测水污染的纤维素3D增强拉曼光谱微流芯片，其特征在于：所述去离子水为0.8%-0.9%w/w。
3.按照权利要求1所述的检测水污染的纤维素3D增强拉曼光谱微流芯片，其特征在于：第二步中，采用浓度为2%w/v的氢氧化钠溶液，水浴温度为80°C，搅拌时间为3h。
4.按照权利要求1所述的检测水污染的纤维素3D增强拉曼光谱微流芯片，其特征在于：第三步中，采用的羧化壳聚糖1g，醋酸50ml，温度为60°C，搅拌60min。
5.按照权利要求1所述的检测水污染的纤维素3D增强拉曼光谱微流芯片，其特征在于：第四步中，1mol/L的硝酸银、1mol/L的硼氢化钠溶液各5ml，均提前15min制备以保持新鲜。
6.权利要求1—5中任一项所述的检测水污染的纤维素3D增强拉曼光谱微流芯片的应用，其特征在于：将污水通入检测水污染的纤维素3D增强拉曼光谱微流芯片中，再对吸附后的微流控芯片进行SERS检测。
7.按照权利要求6所述的检测水污染的纤维素3D增强拉曼光谱微流芯片的应用，其特征在于：SERS检测采用的拉曼激光波长633nm，积分时间为20s，拉曼检测参数为0.7MW。
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